Process for obtaining oxid of titanium from materials incorporating other substances.



omy and perfection than UNITED- STATES PATENT OFFICE.

L OUIB E. BARTON, OF NIAGARA FALLS, ALLOY MANUFACTURING COMPANY, MAINE- NEW Yonx, asszenoa To run 'rrramum or new YORK, N. Y., a coarona'rxon or PROCESS FOR OBTAINING 0111) OF. TITANI'C'M FROM. MATERIALS INCOBPCBATING OTHER SUBSTANCES.

No Drawing.

To all whom it may concern:

Be it known that I, Lows E. BARTCN, a citizen of the United States, and a resident of Niagara Falls, in the county of Niagara and State of New York, have myented a new and useful Process for Obtaining O x1d of Titanium from Materials Incorporat ng other Substances, of which the following is a specification.

This invention relates to the separation, or concentration, of the oxid of titamum from materials containing the same entangled with undesired substances, 1ncludmg compounds of other metals, and its ob ects comprise so doing with ater ease, econeretofore, .the resulting final products consisting, except negli 'bly, of the titanic oxid desired.

e distinctive essentials of the process are as followsrThe material contammg the titanic substance is dissolved in any appropriate, or available, acid, such, for example, as sulfuric hydro-fluoric, or hydrochloric. Throu h the resulting solution, preferably dilu to contain a relatively low ,percentage of said 'oxid, is then passed a current of e ectricity the solution 'being meanwhile heated below boiling. This results in precipitation of a hydrated compound of titamum, the which preci itate is thus obtained without addition to t e solution of alkalis, etc., and, being filtered out and calcined to complete dehydration, yields normally a fina product consisting solely of the titanic oxid, or, exceptionally, only negligibly contaminated.

The process is well adapted to the obtaining of essentially pure titanic oxid from materials such as ores, or concentrates containing therewith -entangled undesired substances such as gangue, or compounds of metals other than titanium a. g. iron compounds. As thus employed, the process is,

or example, practised as follows: Any

titaniferous material, such as titauiferous iron ore, ilmenite, rutile, or preferably, on account of its greater plurity, the titanic acid product of the met 0d described and claimed in Letters Patent No. 1,171542, granted to Auguste Rossi and myself liebruary 15, 1916, is dissolved 1n acid, in this instance, preferably, sulfuric acid.

Specification of Letters Intent.

- said Patented Aug. 7, 1917.

Application filed larch 80, 1917. Serial No. 158,527.

This solution is then, as a catholyte, charged in the cathode compartment of a diphragmed electf'olytic cell, into the anode compartment of which is charged an suitable acid solution in this instance pre erably a sulfuric acid solution. Electrodes, preferably of lead, or of any other substance, or substances capable of, under the conditions, resisting the action of the electrol tes during the electrolysis, are employed. he current bein then turned on and continued, sulfuric acid=will accumulate in the anode, and correspondingly diminish in the cathode, compartment and the catholyte being meanwh' e or thereafter, heated u to preferably 90 to 95 0., there will be therein precipitated, and on several accounts advan tageously, a hydrated compound of titanium, 1'. e. a metatitanic acid compound, for example, basic titanic sulfate, instead of an orthotitanic acid or the like product. The current conditions may be ,varied considerably, but from 5 to 10 volts, and of a current densit of about 30 amperes per square foot, will give satisfactory results.

As to temperatures employed in the heatin passable results are sometimes obtainab e from a little lower temperatures than those above indicated, and also from higher, even up to boiling, though these are rarely, if ever, desirable in practice. In some cases the required heating1 may be more conveniently applied to t e solution withdrawn from the cell after the electrolysis.

It seems that the effect of the electrolysis is to concentrate the titanic oxid and the sulfuric acid in their respective compartments and to maintain the iron, if any present, in ferrous state, and consequently in solution.

In actual o erations there have been thus obtained iel s in precipitates of from 85% to 95% o the tota titanic oxid in the solution, in from two and a half to five hours, but the time required will, of course, in each specific instance, depend u on temperature and current conditions. T e acid accumulated in the anode compartment, as aforeis in con uence readily recoverable.

The resulting ydrated precipitates are as usual, filtered out and dried, and are 0 exceptional value for many uses in the arts,

being devoid of iron and other impurities except negligibly.

To reduce these precipitate products to oxid form, it is necessary only to calcine them to substantially complete dehydration at say about 750 C.

I am aware that Letters Patent No. 758,710, granted to Howard Spence May 3rd, 1904, pur ort to disclose the reduction of titanic sul ate solutions to titanous sulfate solutions by aid of using the former as a catholyte and thereby electrolyzing it in a dia hragm cell, and this step I do not wish to understood as constituting, by itself, any part of my invention, or as covered by m herein claim.

aving now described my invention, what I claim as new and desire to secure by Letters Patent is the following, viz:

The method of obtaining the oxid of titanium from material containing it entangled with undesired substances which comprises dissolving the said material in a suitable acid, electrol zing the resulting solution in the catho e compartment of a diaphragmed electrolytic cell the anode compartment of which contains an acid solution,

eating the resulting catholyte solutiomwitlhdrawing. the resulting precipitated hydrated compound of titanium and calcinin it.

LOUIS E. BA TON.

Witnesses:

Tom C. GRAHAM, RALPH S. TABOR. 

